Amphetamine Synthesis of 1-phenyl-2-nitropropene (P2NP) from benzaldehyde and nitroethane. Henry's reaction.

[ireshop]

Reaction Scheme:

Laboratory equipment and supplies:

• 10 L flask.
• Retort stand and clamp to secure the apparatus (optional).
• Reflux condenser.
• Funnel.
• Vacuum pump.
• Laboratory balance (suitable for 0.1-500 g) - optional.
• 1000 mL and 100 mL measuring cylinders.
• Water bath.
• Glass rod and spatula.
• Filter paper.
• Laboratory thermometer.
• Buchner flask and funnel.
• Bucket of 5-10 L.
• Freezer.

Reagents:

• Benzaldehyde 1000 ml.
• Nitroethane 1000 ml.
• Glacial acetic acid 250 ml.
• n-Butylamine 50 ml.
• Isopropyl alcohol (IPA) ~1000 ml.

Medium scale:

1. Benzaldehyde 1000 ml, nitroethane 1000 ml, glacial acetic acid 250 ml and n-butylamine 50 ml are placed in a 10 L flask.
2. A reflux condenser is installed in the flask.
3. The stirrer and heater are turned on. The reaction mixture is heated to 60 °С.
4. The reaction is carried out for 2-3 hours with constant stirring at 60 °С.
5. The reaction mixture is poured into an empty 5-10 L bucket.
6. 800 ml of IPA is poured into the bucket and stirred.
7. The bucket with the mixture is placed in a freezer for 12 hours, crystallizing 1-phenyl-2-nitropropene (P2NP).
8. The P2NP product is filtered in a Buchner funnel (suction filtration procedure), washed with a small amount of cold IPA and air dried (or in vacuum chamber, optional).

Equipment and glassware:

• 500 ml beaker;
• Funnel;
• Vacuum source;
• Laboratory balance (suitable for 0.1-500 g) - optional;
• 50 mL and 100 mL measuring cylinders;
• Glass rod and spatula;
• Filter paper;
• Buchner flask and funnel;
• Freezer;
• 750 W microwave oven;

Reagents:

• Benzaldehyde 100 ml;
• Nitroethane 100 ml;
• Glacial acetic acid 25 ml;
• n-Butylamine 20 ml;
• Isopropyl alcohol (IPA) ~150 ml;

Small scale (microwave):

1. Benzaldehyde 100 ml, nitroethane 100 ml, glacial acetic acid 25 ml and n-butylamine 20 ml are placed in a 500 ml beaker.
2. A rubber glove is placed in the beaker.
3. The beaker is placed in the microwave.
4. The power of the microwave is set to 750 W. It is turned on and the mixture is heated to boiling. It then cools to room temperature.
5. Repeat step 4 several times. At least 6 times total.
6. Then, 100 ml of IPA is added, the reaction mixture is stirred and placed in a freezer for 12 hours. The 1-phenyl-2-nitropropene (P2NP) is crystallized.
7. The P2NP product is filtered in a Buchner funnel (suction filtration procedure), washed with a small amount of cold IPA and air dried (or in a vacuum chamber, optional).

Re-crystallization of 1-phenyl-2-nitropropene (P2NP) 1-phenyl-2-nitropropene (P2NP) can be recrystallized from hexane, methanol, ethanol or isopropyl alcohol (IPA).